SU213823A1 - - Google Patents
Info
- Publication number
- SU213823A1 SU213823A1 SU1043458A SU1043458A SU213823A1 SU 213823 A1 SU213823 A1 SU 213823A1 SU 1043458 A SU1043458 A SU 1043458A SU 1043458 A SU1043458 A SU 1043458A SU 213823 A1 SU213823 A1 SU 213823A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- tetrachloropropene
- pentachloropropane
- yield
- synthesis
- temperature
- Prior art date
Links
- 238000000034 method Methods 0.000 description 7
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 3
- 235000005074 zinc chloride Nutrition 0.000 description 3
- 239000011592 zinc chloride Substances 0.000 description 3
- FTCVHAQNWWBTIV-UHFFFAOYSA-N 1,1,1,2,2-pentachloropropane Chemical compound CC(Cl)(Cl)C(Cl)(Cl)Cl FTCVHAQNWWBTIV-UHFFFAOYSA-N 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000007033 dehydrochlorination reaction Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- ZXPCCXXSNUIVNK-UHFFFAOYSA-N 1,1,1,2,3-pentachloropropane Chemical compound ClCC(Cl)C(Cl)(Cl)Cl ZXPCCXXSNUIVNK-UHFFFAOYSA-N 0.000 description 1
- GVVUPGXFVJLPDE-UHFFFAOYSA-N 1,3,3,3-tetrachloroprop-1-ene Chemical compound ClC=CC(Cl)(Cl)Cl GVVUPGXFVJLPDE-UHFFFAOYSA-N 0.000 description 1
- FALCMQXTWHPRIH-UHFFFAOYSA-N 2,3-dichloroprop-1-ene Chemical compound ClCC(Cl)=C FALCMQXTWHPRIH-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000008262 pumice Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Description
Изобретение относитс к области получёни 1,1,2,3-тетрахлорПропена-1 исходного продукта дл синтеза селективного гербицида против овсюга-диптала.The invention relates to the field of 1,1,2,3-tetrachloropropena-1 of a starting material for the synthesis of a selective herbicide against oat-diptal.
Известны методы синтеза этого хлорида на Основе товарного 1,1,1,3-тетрахлорпропена путем последовательного проведени стадий деГидрохлорировани и хлорировани , а также метод синтеза, заключающийс в хлорировании 2,3-дихлорпропена газообразным хлором в присутствии азобисизобутиронитрила . При этом требуетс очистка образующихс токсичных сточных вод, кроме того, способ сопровождаетс образованием побочного продукта 1,1,1,2-тетрахлорпропена-2.There are known methods for the synthesis of this chloride on the basis of commodity 1,1,1,3-tetrachloropropene by sequentially carrying out the steps of dehydrochlorination and chlorination, as well as the synthesis method consisting in chlorination of 2,3-dichloropropene with chlorine gas in the presence of azobisisobutyronitrile. This requires purification of the toxic wastewater generated, in addition, the method is accompanied by the formation of a byproduct of 1,1,1,2-tetrachloropropene-2.
Предложенный способ свободен от этих недостатков и более прост в аппаратурном оформлении.The proposed method is free from these disadvantages and more simple in hardware design.
Способ заключаетс в дегидрохлорировании пентахлорпропана в паровой фазе над катализатором (хлористый цинк, осажденный на пористом носителе) при температуре 300-500°С с образованием конечного продукта без примесей изомерного 1,1,2,3-тетрахлорпропена-2 , выход 85%.The method consists in dehydrochlorinating pentachloropropane in the vapor phase over a catalyst (zinc chloride precipitated on a porous carrier) at a temperature of 300-500 ° C to form the final product without isomeric 1,1,2,3-tetrachloropropene-2 impurities, yield 85%.
Пример. В вертикальную трубку, снабженную электрообогревом и термопарой, помещают кусочки пемзы (около 100 мл), пропитанные насыщенным раствором хлористого цинка, и высущнвают их в токе сухого азота при температуре 200°С. Трубку нагревают до 400°С и со скоростью 0,5 мл/мин прикапывают 56 г пентахлорпропана. Выход 1,1,2,3-тетрахлорпропена-1 составл ет 42 гExample. Pumice pieces (about 100 ml) soaked in a saturated solution of zinc chloride are placed in a vertical tube equipped with electrical heating and a thermocouple, and extrude them in a stream of dry nitrogen at a temperature of 200 ° C. The tube is heated to 400 ° C and 56 g of pentachloropropane are added dropwise at a rate of 0.5 ml / min. The yield of 1,1,2,3-tetrachloropropen-1 is 42 g.
(87о/о); т. кип. 68-69°С (30 мм рт. ст); (87o / o); m.p. 68-69 ° С (30 mmHg);
1,5191.1.5191.
Предмет и з о б р е т е и « Subject and reference to the and “
Способ получени 1,1,2,3-тетрахлорпропена-1 путем дегидрохлорировани 1,1,1,2,3-пентахлорпропана при нагревании, отличающийс тем, что, с целью повыщени выхода иThe method of producing 1,1,2,3-tetrachloropropen-1 by dehydrochlorinating 1,1,1,2,3-pentachloropropane with heating, characterized in that, in order to increase the yield and
улучщени качества конечного продукта, упрощени процесса и полного отсутстви сточных вод, процесс дегидрохлорировани провод т в паровой фазе при температуре 300- 500С в присутствии хлористого цинка, осажденного на пористом носителе.improving the quality of the final product, simplifying the process and the complete absence of wastewater, the dehydrochlorination process is carried out in the vapor phase at a temperature of 300-500 ° C in the presence of zinc chloride precipitated on a porous carrier.
Related Child Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU874255320A Addition SU1435923A2 (en) | 1987-04-06 | 1987-04-06 | Method of using heat of waste gases |
| SU874346346A Addition SU1502943A2 (en) | 1987-12-21 | 1987-12-21 | Method of regenerating waste gas heat |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU213823A1 true SU213823A1 (en) |
Family
ID=
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120289751A1 (en) * | 2009-11-27 | 2012-11-15 | Masatoshi Nose | Process for preparing 1,1,2,3-tetrachloropropene |
| WO2017053159A1 (en) | 2015-09-21 | 2017-03-30 | Arkema Inc. | Process for making tetrachloropropene by catalyzed gas-phase dehydrochlorination of pentachloropropane |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120289751A1 (en) * | 2009-11-27 | 2012-11-15 | Masatoshi Nose | Process for preparing 1,1,2,3-tetrachloropropene |
| US8791311B2 (en) * | 2009-11-27 | 2014-07-29 | Daikin Industries, Ltd. | Process for preparing 1,1,2,3-tetrachloropropene |
| WO2017053159A1 (en) | 2015-09-21 | 2017-03-30 | Arkema Inc. | Process for making tetrachloropropene by catalyzed gas-phase dehydrochlorination of pentachloropropane |
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